A new regioselective synthesis of metalinked aromatic polyketones was achieved for the first time. New metaconnected aromatic polyketones with inherent viscosities of up to 0.49 dL/g were regioselectively synthesized by the solution polycondensation of metasubstituted bis(arylsilane)s with aromatic dicarboxylic acid chlorides in the presence of aluminum chloride in 1,2-dichloroethane along with the elimination of chlorotrimethylsilane. The polycondensation proceeded through aromatic electro-philic ipso-substitution. The metalinked aromatic polyketones had considerably lower glass-transition temperatures and 10% weight-loss temperatures than those of their counterpart paracatenated aromatic polyketones. (C) 2003 Wiley Periodicals.